CN109712819A - A kind of KNb3O8Nanometer sheet/carbon cloth composite material preparation method - Google Patents
A kind of KNb3O8Nanometer sheet/carbon cloth composite material preparation method Download PDFInfo
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- CN109712819A CN109712819A CN201811618356.6A CN201811618356A CN109712819A CN 109712819 A CN109712819 A CN 109712819A CN 201811618356 A CN201811618356 A CN 201811618356A CN 109712819 A CN109712819 A CN 109712819A
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- Y02E60/13—Energy storage using capacitors
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Abstract
The invention discloses a kind of KNb3O8Nanometer sheet/carbon cloth composite material preparation method, this method is using the ethanol solution of potassium persulfate and potassium chloride as electrolyte, it is to electrode, saturated calomel electrode as reference electrode to load the carbon cloth after niobium pentoxide nano particle as working electrode, platinized platinum, electrochemical deposition is carried out using cyclic voltammetry, by controlling deposition parameter, the nanometer KNb that size is smaller and is evenly distributed on carbon cloth is obtained3O8Composite material.The KNb that the present invention obtains3O8Nanometer sheet/carbon cloth composite material is when as electrode of super capacitor, with high specific capacitance value, good high rate performance and cyclical stability, and preparation method has the characteristics that route is simple, low in cost, environmental-friendly, there is extremely broad application prospect.
Description
Technical field
The invention belongs to energy storage material technical fields, and in particular to a kind of KNb3O8The preparation of nanometer sheet/carbon cloth composite material
Method.
Background technique
Supercapacitor (Supercapacitor) is a kind of novel energy storage device, because its power density is high, fills
The advantages that velocity of discharge is fast, cyclical stability is excellent and use temperature range is wide, receives the extensive concern of people.Alkali metal niobium
Hydrochlorate (LiNbO3、NaNbO3、KNbO3) there is typical reticular structure, NbO6Octahedron connects in different ways, makes it have
Diversified structure type, but wherein only have calcium to admire mine type (ABO3Type) and pyrochlore-type (A2B2O7Type) two kinds of prototype structures,
He is distorted distortion by both types and is obtained structure type.The structure of matter determines the physicochemical properties of material, therefore, alkali
Metal niobates are a kind of very important multifunctional materials, and there is good ferroelectricity, dielectric, piezoelectricity, photoelectricity, thermoelectricity, light to urge
Change, non-linear optical property, while also having the characteristics that photorefractive effect, low toxicity and chemical stability.In K2O-Nb2O5System
Niobic acid salt compound in niobic acid potassium compound composition it is also extremely complex, the type of compound is more various.Currently, about
K2O-Nb2O5The correlative study of the niobic acid salt compound of system mainly has: KNbO3、KNb4O17、K5.75Nb10.85O30、K3Nb7O19、
K2Nb8O21、KNb3O8Deng.The common synthetic method of niobic acid potassium compound mainly has sol-gel method, solid phase method and hydro-thermal method.It is molten
Glue-gel method is needed using expensive and unstable alkoxide, and operation and reaction must all carry out in dry inert gas atmosphere,
And easily reunited by its powder granule prepared.It is big that hydro-thermal method prepares potassium niobate compounding techniques difficulty, to temperature height,
Reactor pressure size and the concentration of KOH have very high requirement.Product particle partial size made from solid phase method is big, particle size uniformity
Miscellaneous phase is often mixed in difference and product.
Summary of the invention
The object of the present invention is to provide a kind of easy KNb3O8Nanometer sheet/carbon cloth combination electrode material preparation method.
To achieve the above object, the technical solution adopted by the present invention is made of following step:
1, potassium persulfate and potassium chloride are added in ethyl alcohol, stir evenly, obtain electrolyte solution, the electrolyte is molten
Peroxy-disulfuric acid potassium concn is 0.01~1mol/L in liquid, and potassium chloride concentration is 0.01~1mol/L.
2, with nanometer Nb2O5/ carbon cloth combination electrode material is working electrode, platinized platinum be to electrode, saturated calomel electrode is ginseng
It than electrode, is put into the electrolyte solution of step 1, electrochemical deposition is carried out by cyclic voltammetry, depositing temperature is room temperature, work
Making potential section is -1~1V, and sweep speed is 1~50mV/s, and cycle-index is 10~100 times.
3, carbon cloth ultrasonic cleaning, vacuum drying, calcining are taken out after the completion of deposition, obtain KNb3O8Nanometer sheet/carbon cloth composite
Material.
In above-mentioned steps 1, in the electrolyte solution, preferably peroxy-disulfuric acid potassium concn is 0.1~0.5mol/L, potassium chloride
Concentration is 0.1~0.5mol/L.
In above-mentioned steps 2, preferably work potential section is 0~0.45V, and sweep speed is 5~20mV/s, and cycle-index is
40~60 times.
In above-mentioned steps 3, the calcining is 550~800 DEG C of 1~2h of calcining in nitrogen atmosphere, preferably in nitrogen gas
600~700 DEG C of calcining 1h in atmosphere.
Nanometer Nb of the present invention2O5/ carbon cloth combination electrode material is CN108346517A, invention name according to publication No.
Referred to as " nanometer Nb2O5The preparation of method disclosed in the application for a patent for invention of the preparation method of/carbon cloth combination electrode material ".
Beneficial effects of the present invention are as follows:
1, the present invention prepares KNb using electrochemical deposition technique3O8Nanometer sheet/carbon cloth composite material, in gained composite material
KNb3O8Nanometer chip size, content are controllable, even particle size distribution.
2, with previously reported KNb3O8The capacitive property of base electrode is compared, nanometer Nb prepared by the present invention2O5/ carbon cloth is multiple
Flexible electrode material of the condensation material as supercapacitor, in KOH electrolyte have high specific capacitance value, good times it is forthright
Can and and excellent cyclical stability, have in high and new technology field and have been widely used.
3, preparation method of the present invention is simple, time saving and energy saving, and raw material cost is low, nontoxic, environmental-friendly, there is pole
Its broad application prospect.
Detailed description of the invention
Fig. 1 is 1 gained KNb of embodiment3O8Nanometer sheet/carbon cloth composite material XRD diagram.
Fig. 2 is 1 gained KNb of embodiment3O8Nanometer sheet/carbon cloth composite material SEM figure.
Fig. 3 is 1 gained KNb of embodiment3O8The cyclic voltammetric of nanometer sheet/carbon cloth composite material electrode in the case where difference sweeps speed is bent
Line.
Fig. 4 is 1 gained KNb of embodiment3O8Nanometer sheet/carbon cloth composite material electrode under different current densities constant current
Charging and discharging curve.
Fig. 5 is 1 gained KNb of embodiment3O8Nanometer sheet/cyclical stability of the carbon cloth composite material under same current density.
Specific embodiment
The present invention is described in more detail with reference to the accompanying drawings and examples, but protection scope of the present invention is not limited only to
These embodiments.
Nanometer Nb used in following example2O5/ carbon cloth combination electrode material according to publication No. be CN108346517A,
Entitled " nanometer Nb2O5Method system disclosed in the application for a patent for invention of the preparation method of/carbon cloth combination electrode material "
It is standby, it is specific the preparation method is as follows:
Carbon cloth is cut into the size of 1cm × 2cm, acetone, ethyl alcohol is sequentially placed into, is ultrasonically treated 15 points in deionized water
Clock is placed in the HNO for being 68% by 20mL mass fraction after 60 DEG C dry3Aqueous solution and 60mL mass fraction are 98%
H2SO4It in the mixed acid solution of aqueous solution composition, after 100 DEG C of reflow treatment 5h, is cooled to room temperature, takes out and with a large amount of deionizations
Water is rinsed to neutrality, is subsequently placed in 70 DEG C of dry 5h in vacuum oven, the carbon cloth that obtains that treated.It is with niobium oxalate concentration
The aqueous solution that 0.05mol/L, ammonium formiate concentration 0.1mol/L, potassium chloride concentration are 0.5mol/L is electrolyte, after processing
Carbon cloth be working electrode, platinized platinum be to electrode, saturated calomel electrode is reference electrode, electrochemistry is carried out by cyclic voltammetry
Deposition is recycled 2 times, is received wherein the temperature deposited is 70 DEG C, -1.6~0V of work potential section, sweep speed 0.5mV/s
Rice Nb2O5/ carbon cloth combination electrode material.
Embodiment 1
1,1.3g potassium persulfate and 1.1g potassium chloride are added in 100mL ethyl alcohol, stir evenly, it is molten obtains electrolyte
Liquid, in gained electrolyte solution peroxy-disulfuric acid potassium concn be 0.1mol/L, potassium chloride concentration 0.1mol/L.
2, with nanometer Nb2O5/ carbon cloth combination electrode material is working electrode, platinized platinum be to electrode, saturated calomel electrode is ginseng
It than electrode, is put into the electrolyte solution of step 1, electrochemical deposition is carried out by cyclic voltammetry, depositing temperature is room temperature, work
Making potential section is 0~0.45V, and sweep speed 5mV/s, cycle-index is 50 times.
3, carbon cloth deionized water ultrasonic cleaning, 70 DEG C of vacuum drying 5h are taken out after the completion of deposition, then in nitrogen atmosphere
Lower 600 DEG C of calcinings 1h, obtains KNb3O8Nanometer sheet/carbon cloth composite material.
Material obtained above is characterized using x-ray diffractometer, scanning electron microscope etc., the result is shown in Figure 1~
2.As seen from Figure 1, the diffraction maximum position of resulting materials and intensity match with JPCDS card (75-2182), show the material
For KNb3O8.From Figure 2 it can be seen that KNb3O8In nanometer sheet stratiform, and carbon cloth surfaces being evenly distributed on, lateral dimension is about 100~
500nm。
By prepared KNb3O8For nanometer sheet/carbon cloth composite material as working electrode, saturated calomel electrode is reference electricity
Pole, platinum electrode are, in the chemical property of 3mol/L KOH aqueous solution test electrode, as a result to see Fig. 3~5 to electrode.By Fig. 3~
5 as can be seen that KNb3O8Nanometer sheet/carbon cloth composite material is in 2mA/cm2And 50mA/cm2Area specific capacitance point under current density
It Wei not 1844mF/cm2And 981mF/cm2, capacity retention 53% shows excellent cyclical stability.
Embodiment 2
In the present embodiment, 3.9g potassium persulfate and 3.3g potassium chloride are added in 100mL ethyl alcohol, stirs evenly, obtains
Electrolyte solution, in gained electrolyte solution peroxy-disulfuric acid potassium concn be 0.3mol/L, potassium chloride concentration 0.3mol/L.Other
Step is same as Example 1, obtains KNb3O8Nanometer sheet/carbon cloth composite material.Electrochemistry is carried out according to the method for embodiment 1
It can test, gained composite material is in 2mA/cm2High specific capacitance under current density is up to 610mF/cm2, and show preferably
High rate performance, in 50mA/cm2Specific capacitance value under current density is 522mF/cm2, it is the former 85%.
Embodiment 3
In the step 2 of the present embodiment, sweeping speed is 1mV/s, other steps are same as Example 1, obtain a nanometer Nb2O5/ carbon cloth
Composite material.Electrochemical property test is carried out according to the method for embodiment 1, and gained composite material is in 2mA/cm2Under current density
High specific capacitance up to 556mF/cm2, and preferable high rate performance is shown, in 50mA/cm2Ratio electricity under current density
Capacitance is 430mF/cm2, it is the former 77%.
Claims (5)
1. a kind of KNb3O8Nanometer sheet/carbon cloth composite material preparation method, it is characterised in that:
(1) potassium persulfate and potassium chloride are added in ethyl alcohol, stir evenly, obtains electrolyte solution, the electrolyte solution
Middle peroxy-disulfuric acid potassium concn is 0.01~1mol/L, and potassium chloride concentration is 0.01~1mol/L；
(2) with nanometer Nb2O5/ carbon cloth combination electrode material is working electrode, platinized platinum be to electrode, saturated calomel electrode is reference
Electrode is put into the electrolyte solution of step (1), carries out electrochemical deposition by cyclic voltammetry, depositing temperature is room temperature, work
Making potential section is -1~1V, and sweep speed is 1~50mV/s, and cycle-index is 10~100 times；
(3) carbon cloth ultrasonic cleaning, vacuum drying, calcining are taken out after the completion of deposition, obtain KNb3O8Nanometer sheet/carbon cloth composite material.
2. KNb according to claim 13O8Nanometer sheet/carbon cloth composite material preparation method, it is characterised in that: the electricity
Peroxy-disulfuric acid potassium concn is 0.1~0.5mol/L in electrolyte solution, potassium chloride concentration is 0.1~0.5mol/L.
3. KNb according to claim 13O8Nanometer sheet/carbon cloth composite material preparation method, it is characterised in that: in step
(2) in, work potential section is 0~0.45V, and sweep speed is 5~20mV/s, and cycle-index is 40~60 times.
4. KNb according to claim 13O8Nanometer sheet/carbon cloth composite material preparation method, it is characterised in that: in step
(3) in, the calcining is 550~800 DEG C of 1~2h of calcining in nitrogen atmosphere.
5. KNb according to claim 43O8Nanometer sheet/carbon cloth composite material preparation method, it is characterised in that: in step
(3) in, the calcining is 600~700 DEG C of calcining 1h in nitrogen atmosphere.
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| CN201811618356.6A CN109712819B (en) | 2018-12-28 | 2018-12-28 | KNb3O8Preparation method of nanosheet/carbon cloth composite material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112362713A (en) * | 2020-11-24 | 2021-02-12 | 吉林大学 | Sensitive electrode material for direct electrochemical detection of ammonia nitrogen in water and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107204453A (en) * | 2017-05-23 | 2017-09-26 | 宁波大学 | A kind of KNb3O8The preparation method of nanometer rods |
| CN108346517A (en) * | 2018-02-06 | 2018-07-31 | 陕西师范大学 | Nanometer Nb2O5The preparation method of/carbon cloth combination electrode material |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107204453A (en) * | 2017-05-23 | 2017-09-26 | 宁波大学 | A kind of KNb3O8The preparation method of nanometer rods |
| CN108346517A (en) * | 2018-02-06 | 2018-07-31 | 陕西师范大学 | Nanometer Nb2O5The preparation method of/carbon cloth combination electrode material |
Non-Patent Citations (1)
| Title |
|---|
| HIDEKI NAKAYAMA等: ""Electrochemical reactions of layered niobate material as novel anode for sodium ion batteries"", 《JOURNAL OF POWER SOURCES》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112362713A (en) * | 2020-11-24 | 2021-02-12 | 吉林大学 | Sensitive electrode material for direct electrochemical detection of ammonia nitrogen in water and preparation method thereof |
| CN112362713B (en) * | 2020-11-24 | 2021-12-07 | 吉林大学 | Sensitive electrode material for direct electrochemical detection of ammonia nitrogen in water and preparation method thereof |
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